Characterisation Methods in Solid State and Materials Science

PRELIMS.pdf
Author biography
Kelly Morrison
CH001.pdf
Chapter 1 Introduction
1.1 Overview
1.2 Microscopy, spectroscopy and diffraction
1.3 Introductory optics
1.3.1 Definitions of a wave
1.3.2 Refraction, reflection, retardation
1.3.3 Diffraction
1.3.4 Resolution
1.3.5 Lenses
1.4 Introduction to atomic physics
1.4.1 The periodic table
1.4.2 The photoelectric effect
1.4.3 The atomic model, and energy levels
1.5 Introductory solid state physics
1.5.1 The crystal lattice
1.5.2 Translation vectors
1.5.3 Miller indices and notation
1.5.4 Wyckoff sites and space groups
References
CH002.pdf
Chapter 2 Fourier series, transforms and their relevance in diffraction and microscopy
2.1 Introduction
2.2 Fourier series
2.3 The Fourier transform
2.4 Key functions and their Fourier transforms
2.4.1 The aperture function (single slit of finite width)
2.4.2 The Dirac delta function (infinitely narrow slit)
2.4.3 The Lorentzian and Gaussian functions
2.5 The convolution theorem
2.6 Classic examples of diffraction patterns
2.6.1 Young’s double slit
2.6.2 The diffraction grating
2.7 Autocorrelation and the loss of phase information in measurements
2.8 Aside: some useful theorems
2.8.1 Linearity theorem
2.8.2 Scaling theorem
2.8.3 Shifting theorem
2.8.4 Parseval’s theorem
2.8.5 Correlation theorem
2.8.6 Convolution theorem
2.9 Questions
2.9.1 Some standard Fourier transforms
2.9.2 Normalisation of the Fourier transform pair
2.9.3 Further questions
References
CH003.pdf
Chapter 3 Diffraction techniques
3.1 Elastic scattering
3.1.1 X-rays versus neutrons
3.1.2 Nuclear scattering length and form factors
3.1.3 Scattering cross-section
3.1.4 Some final notes
3.2 Methods
3.2.1 X-ray sources
3.2.2 Neutron sources
3.2.3 Time of flight
3.2.4 Detectors
3.3 Diffraction: Rietveld refinement
3.3.1 Least squares refinement
3.3.2 General equation
3.3.3 Structure factor
3.3.4 Profile function
3.3.5 Basic refinement strategy
3.3.6 Figures of merit
3.3.7 Single crystal diffraction
3.3.8 Magnetic contrast
3.4 Grazing incidence diffraction
3.5 X-ray and neutron reflectivity (XRR & NR)
3.5.1 Overview
3.5.2 Fourier derivation of the reflectivity curve
3.5.3 Classic examples of reflectivity profiles
3.5.4 X-rays versus neutrons
3.5.5 Polarised neutron reflectivity (PNR)
3.6 Examples of diffraction techniques in the literature
3.6.1 In ‘Strain in nanoscale germanium hut clusters on Si(001) studied by x-ray diffraction’
3.6.2 In ‘Neutron-diffraction study of the Jahn–Teller transition in stoichiometric LaMnO3’
3.6.3 In ‘Neutron-diffraction measurements of magnetic order and a structural transition in the parent BaFe2As2 compound of FeAs-based high temperature superconductors’
3.6.4 In ‘Unconventional magnetic order on the hyperhoneycomb Kitaev lattice in β-Li2IrO3: full solution via magnetic resonant x-ray diffraction’
3.7 Questions
3.7.1 Structure factor and reflection rules
3.7.2 Extracting key information from x-ray diffraction data
3.7.3 Space groups
3.7.4 Identifying key information in XRR data
3.7.5 Computer aided problems
3.7.6 Calibrating detectors—some basic geometry
References
CH004.pdf
Chapter 4 Microscopy techniques
4.1 Optical microscopy
4.1.1 The optical microscope
4.1.2 Use of polarised light
4.1.3 Phase contrast imaging
4.1.4 Interference contrast microscopy
4.2 Electron microscopy
4.2.1 Scanning electron microscopy (SEM)
4.2.2 Sources
4.2.3 SEM resolution and contrast
4.2.4 Sample preparation and beam damage
4.2.5 Transmission electron microscopy (TEM)
4.3 Profilometry
4.3.1 Optical profilometry
4.3.2 Scanning tunnelling microscope (STM)
4.3.3 Atomic force microscope (AFM)
4.4 Examples of microscopy techniques in the literature
4.4.1 In ‘Atomic-scale structural and electronic properties of SrTiO3/GaAs interfaces: a combined STEM-EELS and first principles study’
4.4.2 In ‘Intermixing and periodic self-assembly of borophene line defects’
4.4.3 In ‘Resolving strain in carbon nanotubes at the atomic level’
4.4.4 In ‘Atomic structure and dynamics of single platinum atom interactions with monolayer MoS2’
References
CH005.pdf
Chapter 5 Spectroscopy techniques
5.1 What is spectroscopy?
5.2 Energy loss spectroscopy
5.2.1 Inelastic neutron spectroscopy (INS)
5.2.2 Raman spectroscopy
5.2.3 Brillouin light scattering spectroscopy (BLS)
5.2.4 Electron energy loss spectroscopy (EELS)
5.3 Electron spectroscopy
5.3.1 Overview
5.3.2 X-ray photoelectron spectroscopy (XPS)
5.3.3 Ultraviolet photoemission spectroscopy (UPS)
5.3.4 Angle resolved photoemission spectroscopy (ARPES)
5.3.5 Auger electron spectroscopy (AES)
5.4 Fluorescence techniques
5.4.1 X-ray fluorescence (XRF)
5.4.2 Energy dispersive x-ray spectroscopy (EDS, EDX, XEDS)
5.5 Absorption spectroscopy
5.5.1 UV-visible absorption spectroscopy
5.5.2 Infrared absorption spectroscopy
5.5.3 X-ray absorption spectroscopy (XAS)
5.5.4 Mössbauer spectroscopy
5.6 Resonance techniques
5.6.1 Nuclear magnetic resonance (NMR)
5.6.2 Electron spin resonance (ESR)
5.6.3 Ferromagnetic resonance (FMR)
5.7 Examples of spectroscopy techniques in the literature
5.7.1 In ‘Magnetic imaging—Snell’s law for spin waves’
5.7.2 In ‘Structural evolution and characteristics of the phase transformations between α-Fe2O3, Fe3O4 and γ-Fe2O3 nanoparticles under reducing and oxidizing atmospheres’
5.7.3 In ‘A new and simple route to prepare γ-Fe2O3 with iron oxide scale’
5.7.4 In ‘Understanding the origin of band gap formation in graphene on metals: graphene on Cu/Ir(111)’
5.7.5 In ‘Experimental realization of a three-dimensional topological insulator, Bi2Te3’
5.7.6 In ‘Magnetostrictive thin films for microwave spintronics’
References
CH006.pdf
Chapter 6 Thermal characterisation
6.1 Some background theory
6.1.1 Temperature scales, heat and the laws of thermodynamics
6.1.2 Transfer of heat
6.1.3 Specific heat, latent heat and phase transitions
6.1.4 Thermal conductivity and interfacial thermal conductance
6.1.5 Measurement of temperature and heat flux
6.2 Calorimetry
6.2.1 Adiabatic calorimetry
6.2.2 Relaxation and hybrid calorimeters
6.2.3 Differential scanning calorimetry (DSC)
6.2.4 Differential thermal analysis (DTA)
6.2.5 Thermogravimetric analysis (TGA)
6.2.6 AC calorimetry
6.2.7 Removal of addenda
6.3 Thermal conductivity
6.3.1 Steady state methods
6.3.2 Transient methods
6.3.3 Thin film methods
6.3.4 Summary
6.4 Examples of thermal characterisation techniques from the literature
6.4.1 In ‘Neutron-diffraction study of the Jahn–Teller transition in stoichiometric LaMnO3’
6.4.2 In ‘Evaluation of the reliability of the measurement of key magnetocaloric properties: a round robin study of La(Fe,Si,Mn)Hδ conducted by the SSEEC consortium of European laboratories’
6.4.3 In ‘Magnetic phase transitions and the magnetothermal properties of gadolinium’
6.4.4 In ‘Low-temperature specific heat and critical magnetic field of α-uranium single crystals’
6.4.5 In ‘Thermal conductivity, electrical resistivity, and Seebeck coefficient of silicon from 100 to 1300 K’
6.4.6 In ‘Reduction of thermal conductivity by surface scattering of phonons in periodic silicon nanostructures’
References
CH007.pdf
Chapter 7 Electric characterisation
7.1 Introduction
7.1.1 Background
7.1.2 Consequences of bandstructure
7.1.3 Types of materials
7.1.4 Bandstructure engineering
7.2 Thermo- and magneto-electric effects
7.2.1 Hall effects
7.2.2 Thermoelectric effects
7.3 Basics of an electric measurement
7.3.1 Measurement of current
7.3.2 Measurement of voltage
7.3.3 Measurement of resistance
7.3.4 Sources of noise
7.3.5 The lock-in amplifier
7.4 Measurement of resistivity
7.4.1 The 4-point probe technique
7.4.2 Magnetoresistance measurements
7.4.3 Hall measurements
7.5 Bandstructure measurements
7.5.1 Point contact spectroscopy
7.5.2 Quantum oscillations
7.6 Examples of electric characterisation techniques in the literature
7.6.1 In ‘Negative Hall coefficient of ultrathin niobium in Si/Nb/Si trilayers’
7.6.2 In ‘Simultaneous detection of the spin-Hall magnetoresistance and the spin-Seebeck effect in platinum and tantalum on yttrium iron garnet’
7.6.3 In ‘Structural, electronic, and magnetic investigation of magnetic ordering in MBE-grown CrxSb2−xTe3 …’
7.6.4 In ‘Transport magnetic proximity effects in platinum’
7.6.5 In ‘Topology-driven magnetic quantum phase transition in topological insulators’
7.7 Questions
7.7.1 Extracting information from bulk measurements
7.7.2 Extracting information from thin film measurements
References
CH008.pdf
Chapter 8 Magnetic characterisation
8.1 Fundamentals of magnetism
8.1.1 Some units
8.1.2 Types of magnetic order
8.1.3 Magnetic domain theory
8.1.4 Demagnetisation effects
8.2 Magnetic interactions
8.2.1 Magnetic dipolar interaction
8.2.2 The exchange integral
8.2.3 Direct exchange
8.2.4 Indirect metallic exchange (RKKY interaction)
8.2.5 Indirect ionic exchange (superexchange)
8.2.6 Double exchange
8.2.7 Anisotropic exchange (Dzyaloshinky–Moriya interaction)
8.3 Magnetometry
8.3.1 Vibrating sample magnetometer (VSM)
8.3.2 SQuID magnetometry
8.3.3 Extraction method
8.4 Magnetic imaging
8.4.1 Magneto-optic Kerr effect (MOKE)
8.4.2 Scanning Hall probe
8.4.3 Magnetic force microscopy (MFM)
8.4.4 Spin polarised scanning tunneling microscopy (SP-STM)
8.4.5 Scanning electron microscopy with polarisation analysis (SEMPA)
8.4.6 Transmission electron microscopy (TEM) methods
8.4.7 Photoexcited electron microscopy (PEEM) and scanning transmission x-ray microscopy (STXM)
8.5 Examples of magnetisation techniques in the literature
8.5.1 In ‘Depth profile of spin and orbital magnetic moments in a subnanometer Pt film on Co’
8.5.2 In ‘Room-temperature helimagnetism in FeGe thin films’
8.5.3 In ‘Direct observation of magnetic monopole defects in an artificial spin-ice system’
8.5.4 In ‘Quantum spin chains with frustration due to Dzyaloshinskii–Moriya interactions’
8.5.5 In ‘Neutron diffraction study of the magnetic properties of the series of Perovskite-type compounds [(1 − x)La,xCa]MnO3’
8.6 Questions
8.6.1 Magnetic units, a quagmire
8.6.2 Magnetic interactions
8.6.3 Extracting information from magnetisation measurements
References
APP1.pdf
Chapter
APP2.pdf
Chapter
APP3.pdf
Chapter
APP4.pdf
Chapter
APP5.pdf
Chapter
APP6.pdf
Chapter
APP7.pdf
Chapter
References
APP8.pdf
Chapter
H.1 Classical diffraction examples
H.2 Test of the shift theorem
H.3 Test of the addition theorem
H.4 Test of the convolution theorem
1.5 Spatial filtering
APP9.pdf
Chapter